CN115010956B - Polytannic acid nanotube material selectively enriched with Pd, application of material in purification and recovery of Pd in waste colloid palladium and preparation method of material - Google Patents

Polytannic acid nanotube material selectively enriched with Pd, application of material in purification and recovery of Pd in waste colloid palladium and preparation method of material Download PDF

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CN115010956B
CN115010956B CN202210653275.XA CN202210653275A CN115010956B CN 115010956 B CN115010956 B CN 115010956B CN 202210653275 A CN202210653275 A CN 202210653275A CN 115010956 B CN115010956 B CN 115010956B
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nts
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CN115010956A (en
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张婷婷
黄渝川
谭夏霖
张立挺
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Hangzhou Lvsaikelin Technology Co ltd
Zhejiang Lover Health Science and Technology Development Co Ltd
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Zhejiang Lover Health Science and Technology Development Co Ltd
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C22B11/042—Recovery of noble metals from waste materials
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Abstract

The invention discloses a poly-tannic acid nanotube material selectively enriched with Pd, and an application and a preparation method of the poly-tannic acid nanotube material in purifying and recycling Pd in waste colloid palladium, and relates to the technical field of precious metal recycling. The poly tannic acid nanotube material is manufactured by taking curcumin as a template, removing the template curcumin after oxidation and self-polymerization of tannic acid on the surface of the material, obtaining the poly tannic acid nanotube TA-NTs with a hollow single-wall structure, which is used for selectively reducing noble metal Pd and enriching the noble metal Pd on the surface, wherein the deposition of dissolved noble metal Pd ions on the poly tannic acid nanotube is realized through a simple green reduction process, and other impurity metals such as common metal ions in electroplating processes of Fe\Ni\Cu\Zn\Pb\Sn and the like are not enriched on the surface of the material, so that the material is a biomass-based tubular new material with the function of selectively reducing the noble metal Pd, and can simplify the noble metal recovery process in colloid palladium and improve the green of the whole process.

Description

Polytannic acid nanotube material selectively enriched with Pd, application of material in purification and recovery of Pd in waste colloid palladium and preparation method of material
Technical Field
The invention relates to the technical field of precious metal recovery, in particular to a poly tannic acid nanotube material selectively enriched with Pd, and an application and a preparation method of the poly tannic acid nanotube material in purifying and recovering Pd in waste colloid palladium.
Background
To effect the connection of electronic components in the electroplated circuit board, the PCB must be perforated and the surface metallized, requiring activation with colloidal palladium. The colloidal palladium is a colloidal solution with atomic palladium as a colloid core and is prepared from PdCl 2 And a reducing agent. The Pd/Sn type colloidal palladium is the most common at present, and is an activator with excellent catalytic performance for the metallization of nonmetallic materials. During the electroplating process, the colloid palladium activating liquid is used for long term and empty of colloid palladium in the tankThe metal oxidant brought in is accumulated for a long time due to gas contact and uncleanness in the plating process, so that coagulation and failure of the colloid palladium activating solution are easy to cause, a large amount of waste colloid palladium activating solution exists, and the method has great significance for recovering palladium metal in the waste colloid palladium due to high price of the palladium metal.
Existing precious metal recovery methods include hydrometallurgical and pyrometallurgical processes such as cementation, adsorption, ion exchange, solvent extraction and electrowinning. Hydrometallurgical processes use leaches to extract noble metal palladium from solid waste sources, which are currently the method of choice for noble metal recovery due to higher noble metal recovery and fully developed and controlled processes. Specifically, the existing hydrometallurgy comprises the following specific process flows: waste colloid palladium, dilution, pH value adjustment, heating gel breaking, filtration, aqua regia dissolution, pH value adjustment and Sn (OH) filtration 4 Repeating precipitation, reduction, sponge palladium (containing metal impurities), refining, and metal palladium. However, the technology still has the obvious defects of poor effect of removing acid-base wastewater and impurity metals, complex technology, high labor intensity and high consumption of reagents and energy. In particular to dissolving in aqua regia, regulating pH value and filtering out Sn (OH) 4 Repeated precipitation, reduction and refining are still required after precipitation, and the operation is complicated and time-consuming.
Disclosure of Invention
In order to simplify the recovery process of noble metals in colloidal palladium and improve the environmental protection of the whole process, the invention provides a poly tannic acid nanotube material selectively enriched with Pd, and an application and a preparation method of the poly tannic acid nanotube material in purifying and recovering Pd in waste colloidal palladium.
The technical scheme adopted by the invention for realizing the technical effects is as follows:
the first object of the present invention is to provide a poly tannic acid nanotube material selectively enriched in Pd, which is produced by using curcumin as a template, removing the template curcumin after oxidation and self-polymerization of tannic acid on the surface of the material, and obtaining the poly tannic acid nanotube TA-NTs with a hollow single-wall structure, wherein the poly tannic acid nanotube material selectively reduces noble metal Pd and enriches the noble metal Pd on the surface.
Preferably, in the above-mentioned selectively Pd-rich polytannin nanotube material, the average external diameter of the polytannin nanotubes TA-NTs is 200 nm and the average wall thickness is about 50 nm.
The second object of the present invention is to provide an application of the selectively Pd-enriched in poly-tannic acid nanotube material in purifying and recovering Pd from waste colloidal palladium, which comprises the following process steps: waste colloid palladium, dilution, pH value adjustment, heating gel breaking, filtration, aqua regia dissolution, pH value adjustment and Sn (OH) filtration 4 Precipitation- & gt poly (tannic acid) nanotubes TA-NTs- & gt metallic palladium.
Preferably, in the above application of the selectively Pd-enriched polytannin nanotube material in purifying and recovering Pd from waste colloidal palladium, the polytannin nanotube TA-NTs is added after Sn (OH) is filtered out 4 In the precipitated wastewater solution, pd (NH) in the wastewater solution is selectively reduced 3 ) 4 Cl 2 Directly obtaining the metal palladium nano particles automatically enriched on the surface of the poly tannic acid nano tube TA-NTs.
A third object of the present invention is to provide a method for preparing a material of a poly tannic acid nanotube selectively enriching Pd as described above, the method comprising the steps of:
s1, dissolving 0.1 g of curcumin in 50 ml of ethanol/acetone mixture;
s2, gradually injecting 800 milliliters of 0.5M BICINE buffer solution into the mixture in the step S1, separating out curcumin linear crystals, and filtering to obtain curcumin crystals;
s3, suspending the curcumin crystals in 100 ml of 0.5M BICINE buffer solution again, adding 1.6 g of tannic acid powder into the mixed solution, and stirring for 3 hours;
s4, centrifugally separating out curcumin@TA-NTs in the step S3 at a rotating speed of 5000rpm, washing with ethanol for 2 times again, and washing with deionized water for one time to remove curcumin;
s5, collecting the tannin nanotube material by using a centrifugal machine, and drying the tannin nanotube material under vacuum.
Preferably, in the above method for preparing a selectively Pd-enriched in poly tannic acid nanotube material, the BICINE buffer has a ph=7.8.
The beneficial effects of the invention are as follows: the invention improves the prior process for purifying and recovering Pd in waste colloid palladium in a green way, and filters Sn (OH) 4 After precipitation, directly adding the poly tannic acid nanotube TA-NTs, and selectively reducing Pd (NH) by using the new material 3 ) 4 Cl 2 The metal palladium nano particles automatically enriched on the surface of the poly tannic acid nano tube TA-NTs are directly obtained, the subsequent repeated technological processes of precipitation, reduction, refining and the like are omitted, and the recovery process of high-purity metal palladium in waste colloidal palladium is greatly simplified.
Drawings
FIG. 1 is a schematic diagram showing the synthesis of TA-NTs of the tannin nanotubes according to the present invention;
FIG. 2 is a transmission electron microscope image of the TA-NTs of the tannin nanotubes of the present invention;
FIG. 3 is a transmission electron microscope image of TA-NTs enriched in palladium metal in the invention;
FIG. 4 is a Raman spectrum comparison chart of TA-NTs and TA-NTs-Pd in the invention;
FIG. 5 is an XRD pattern for TA-NTs and TA-NTs-Pd in the present invention;
FIG. 6 is a graph showing the effect of selective enrichment of Pd on TA-NTs by the tannin nanotubes of the present invention.
Detailed Description
The present invention will be described more fully hereinafter in order to facilitate an understanding of the present invention. This invention may be embodied in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
It is to be understood that the weight of the relevant components mentioned in the embodiments of the present invention may refer not only to the specific content of each component, but also to the proportional relationship between the weights of the components, so long as the content of the relevant components is scaled up or down in accordance with the embodiments of the present invention, which is within the scope of the present disclosure. Specifically, the weight in the embodiment of the invention can be mass units well known in the chemical industry field such as mu g, mg, g, kg.
In addition, the expression of a word in the singular should be understood to include the plural of the word unless the context clearly indicates otherwise. The terms "comprises" or "comprising" are intended to specify the presence of stated features, integers, steps, operations, elements, components, or groups thereof, but are not intended to preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, or groups thereof.
In order that the details of the above-described implementations and operations of the present invention may be clearly understood by those skilled in the art, and that the present invention may be embodied with significant improvements in the embodiments of the present invention, the above-described technical solutions will be exemplified by a plurality of embodiments.
In a first aspect, embodiments of the present invention provide a selectively Pd-enriched poly-tannic acid nanotube material, which is produced using curcumin as a template, and removing the template curcumin after oxidation and autopolymerization of tannic acid on the surface thereof, to obtain a poly-tannic acid nanotube TA-NTs having a hollow single-wall structure with selectively reduced noble metal Pd and enriched on the surface. Specifically, in a preferred embodiment of the present invention, the average external diameter of the poly-tannic acid nanotubes TA-NTs is 200 nm and the average wall thickness is about 50 nm.
Tannic Acid (TA) is a natural plant-derived polyphenol that has been demonstrated to interact with molecules as a surrogate and deposit on the surface of almost all types of solid materials, producing a large number of reactive hydroxyl, amine and azurin groups. According to the invention, curcumin is taken as a template to manufacture the poly-tannic acid nanotube TA-NTs selectively enriched with Pd, and the template curcumin is removed after oxidation and self-polymerization of Tannic Acid (TA) on the surface of the poly-tannic acid nanotube TA-NTs to obtain the poly-tannic acid nanotube TA-NTs with a hollow single-wall structure. The deposition of dissolved noble metal pd ions on the poly-tannic acid nanotubes TA-NTs can be realized through a simple green reduction process, and other impurity metals such as common metal ions in electroplating processes of Fe\Ni\Cu\Zn\Pb\Sn and the like can not be enriched on the surface of the material, and the tubular structure can further increase the enrichment area of noble metals. Therefore, the poly tannic acid nanotube TA-NTs provided by the invention is a biomass-based tubular new material with the function of selectively reducing noble metal Pd.
The second object of the present invention is to provide an application of the selectively Pd-enriched in poly-tannic acid nanotube material in purifying and recovering Pd from waste colloidal palladium, which comprises the following process steps: waste colloid palladium, dilution, pH value adjustment, heating gel breaking, filtration, aqua regia dissolution, pH value adjustment and Sn (OH) filtration 4 Precipitation- & gt poly (tannic acid) nanotubes TA-NTs- & gt metallic palladium.
Specifically, in the examples of the present invention, the addition of the poly-tannic acid nanotubes TA-NTs resulted in the filtration of Sn (OH) 4 In the precipitated wastewater solution, pd (NH) in the wastewater solution is selectively reduced by using a poly tannic acid nanotube TA-NTs 3 ) 4 Cl 2 Directly obtaining the metal palladium nano particles automatically enriched on the surface of the poly tannic acid nano tube TA-NTs. As shown in FIG. 3, a transmission electron microscope plot shows metal palladium nanoparticles enriched on the surface of the tube body of the poly-tannic acid nanotubes TA-NTs, with a particle size of 20-100nm.
A third object of the present invention is to provide a method for preparing the above-mentioned selectively Pd-enriched in a poly-tannic acid nanotube material, comprising the steps of:
s1, dissolving 0.1 g of curcumin in 50 ml of ethanol/acetone mixture;
s2, gradually injecting 800 milliliters of 0.5M BICINE buffer solution into the mixture in the step S1, separating out curcumin linear crystals, and filtering to obtain curcumin crystals;
s3, suspending the curcumin crystals in 100 ml of 0.5M BICINE buffer solution again, adding 1.6 g of tannic acid powder into the mixed solution, and stirring for 3 hours;
s4, centrifugally separating out curcumin@TA-NTs in the step S3 at a rotating speed of 5000rpm, washing with ethanol for 2 times again, and washing with deionized water for one time to remove curcumin;
s5, collecting the tannin nanotube material by using a centrifugal machine, and drying the tannin nanotube material under vacuum.
Specifically, in an embodiment of the present invention, the BICINE buffer has a ph=7.8.
When practical verification is carried out, firstly, the multi-element ICP standard solution is used for researching the metal selective adsorption and enrichment performance of TA-NTs. Wherein the standard solution is (Fe, ni, cu, zn, pb, sn, ag, pd in 5% HCL and 1% HNO 3 In (c) a). The method comprises the following specific steps: the poly tannic acid nanotube TA-NTs (100 mg/mL) prepared by the method is dispersed in 10mL of mixed standard solution containing 100ppb of various metal substances, and then is oscillated for 3 hours, and then is centrifuged through a 0.2 micrometer membrane. Finally, the content of each metal ion in the filtered liquid was measured by inductively coupled plasma mass spectrometry (ICP-MS). The concentration of each metal ion before and after the adsorption of the TA-NTs of the poly-tannin nanotubes is changed to determine the selective enrichment of the TA-NTs of the poly-tannin nanotubes on the metal ions. Specific measurement results are shown in fig. 3 to 6, wherein fig. 3 is a transmission electron microscope diagram of TA-NTs-Pd in the invention, the particle size of 20-100nm is palladium metal nano particles adsorbed in the diagram, fig. 4 is a raman spectrum contrast diagram of TA-NTs and TA-NTs-Pd in the invention, and fig. 5 is an XRD contrast diagram of TA-NTs and TA-NTs-Pd in the invention, which can both indirectly or directly illustrate the enrichment of palladium metal in the diagram; 6 is an effect diagram of selective enrichment of Pd by TA-NTs in the invention, and can also be seen that TA-NTs show remarkable selective enrichment effect in a mixed solution in which a plurality of metal ions exist simultaneously.
In conclusion, the invention improves the prior purification and recovery of Pd from waste colloidal palladium in a green way, and filters Sn (OH) 4 After precipitation, directly adding the poly tannic acid nanotube TA-NTs, and selectively reducing Pd (NH) by using the new material 3 ) 4 Cl 2 The metal palladium nano particles automatically enriched on the surface of the poly tannic acid nano tube TA-NTs are directly obtained, the subsequent repeated technological processes of precipitation, reduction, refining and the like are omitted, and the recovery process of high-purity metal palladium in waste colloidal palladium is greatly simplified.
The above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention, and are intended to be included in the scope of the present invention.

Claims (6)

1. The preparation method of the poly tannic acid nanotube material selectively enriched with Pd is characterized by comprising the following steps:
s1, dissolving 0.1 g of curcumin in 50 ml of ethanol/acetone mixture;
s2, gradually injecting 800 milliliters of 0.5MBICINE buffer solution into the mixture in the step S1, separating out curcumin linear crystals, and filtering to obtain curcumin crystals;
s3, suspending the curcumin crystals in 100 ml of 0.5MBICINE buffer solution again, adding 1.6 g of tannic acid powder into the mixed solution, and stirring for 3 hours;
s4, centrifugally separating out curcumin@TA-NTs in the step S3 at a rotating speed of 5000rpm, washing with ethanol for 2 times again, and washing with deionized water for one time to remove curcumin;
s5, collecting the tannin nanotube material by using a centrifugal machine, and drying the tannin nanotube material under vacuum.
2. The method of claim 1, wherein the BICINE buffer has a ph=7.8.
3. A material of a poly tannic acid nanotube selectively enriched with Pd, characterized in that it is produced using curcumin as a template according to the method of claim 1 or 2, and the template curcumin is removed after oxidation self-polymerization of tannic acid on the surface thereof, and the obtained poly tannic acid nanotube TA-NTs having a hollow single wall structure selectively reducing noble metal Pd and enriching it on the surface.
4. The selectively Pd-rich in poly (tannic acid) nanotube material of claim 3, wherein the average external diameter of the poly (tannic acid) nanotubes TA-NTs is 200 nm and the average wall thickness is 50 nm.
5. The use of the selectively Pd-enriched in-poly-tannic acid nanotube material prepared by the method of claim 1 or 2 to purify and recover Pd from spent colloidal palladium, wherein: the method comprises the following process flows: waste colloid palladium, dilution, pH value adjustment, heating gel breaking, filtration, aqua regia dissolution, pH value adjustment and Sn (OH) filtration 4 Precipitation- & gt poly (tannic acid) nanotubes TA-NTs- & gt metallic palladium.
6. The use of the selectively Pd-rich polyglutamic acid nanotube material of claim 5 for purifying and recovering Pd from spent colloidal palladium, wherein: the addition of the poly tannic acid nano tube TA-NTs filters out Sn (OH) 4 In the precipitated wastewater solution, pd (NH) in the wastewater solution is selectively reduced 3 ) 4 Cl 2 And ions are directly obtained to obtain metal palladium nano particles automatically enriched on the surface of the poly tannic acid nano tube TA-NTs.
CN202210653275.XA 2022-06-09 2022-06-09 Polytannic acid nanotube material selectively enriched with Pd, application of material in purification and recovery of Pd in waste colloid palladium and preparation method of material Active CN115010956B (en)

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